Manufacture of pure carbon.



H. HENNEBUTTE- MANUFACTURE OF PURE CARBON.

APPLICATION FLLED FEB. 2|. I914.

1,155,419. Patented Oct. 5, 1915.

INVENTOR WITNESSES I 1 BY W 56 4 AifORNEY UNTTED STATES PATENT OFFICE.

HENRI HENNEBUTTE, 0F PARIS, FRANCE, ASSIGNOR TO SOCIETE ANONYME DESCOMBUSTIBLES INDUSTRIELS, OF PARIS, FRANCE.

MANUFACTURE OF PURE CARBON.

Specification of Letters Patent.

Patented Oct. 5, 1915.

To all lit/mm it may concern:

lie it known that I, l-lsum Hsxsaau'rrs, citizen of France. residing at25 Rue Pigalle. Paris, France, have invented certain new and usefulImpro eim-nts in the Manufacture of Pure Carbon, of which the followingis a specifi at on.

This invention relates to a process for the umuufacture of a materialcontaining a cer tain proportion of pure carbon that can be used for any)urposes, but is intended chiefly for electrical purposes, said materialbeing obtained by usin hydrocarbons such as coal tar and tar oi spetroleum tar or oils and various other hydrocarbons, in fact anyorganic material. that is rich in carbon and contains hilt little ashand that either alone or mixed with other organic substances is liquidbelow 200 C.

The process consists in first removing-any mineral dust that may becontained inithe-- material to be treated, this removal being effectedeither by allowing the material to stand or by filtration. Thehydrocarbon or tar oil that constitutes the raw material is thensimultaneously heated and submitted to the action of a current of air oroxidizing gas supplied in a well divided condition and for aconsiderable length of time. This current of air or oxidizing gas isintended to dehydrogenate the hydrocarbon and produce stronglydehydrogenated substances that. by subsequent carbonization will yield asubstantial proportion of pure graphiteliku carbon. The air will betternot on the hydrocarbons when the hydrocarbons are sprayed into contactwith the air, since it increases their contact with the air, or thehydrocarbons may be passed in a gaseous or vaporous state into a heatedreceiver and be therein treated with a current of air or oxidizinggaseous matter. In order to render the transformation of the hydrocarbonor tar oil more complete and rapid the static pressure of the mass ofoil or tar under treatment can be increased. The action of the heat andthat of the oxidizing gas must be stopped before carbonization of thewhole mass begins to set in, i. (2. before the material becomes coked(between 400 and 500 C.) The material or mass obtained in this manner issubmitted to the action of a solvent, such as benzene, petroleum oils ortar oils, in order to separate the insoluble portion of the rilaterialconsisting of strongly dehydrogcnated substances from the solubleportion. The insoluble part referred to is removed by decanting orfiltering the oxidized mass of oil, and is submitted to the action ofheat until it is thoroughly carbonized, the pure carbon to he producedbeing obtained in this manner.

The carbon secured by this process is hard and resembles graphite. It isbut slightly porous and may serve as a good conductor of electricity. Itcan advantageously be used for the manufacture of electrodes and otherelectric conductors.

As regards the part of the oxidized mass obtained by mixing the oilswith the soluble substances of the original material, the same isdistilled in order to separate oil the solvent. On having thusrecuperated the solvent in a known manner by distillation, the dissolvedsubstances obtained as a residue are a ain submitted, either alone ormixed witi a further amount of raw material, to the oxidation abovereferred to, until these substances are likewise transformed into astrongly dehydrogenated insoluble mass.

Reference is now to be had to the accompanying drawing illustrating byway of example, an apparatus which may be used to practise the process.

The hydrocarbon to be treated is preferably left standing or filtered orotherwise threated so as to remove mineral dust which may be present,and is then either in a liquid or gaseous state supplied through a pipe1 to a reservoir or still 2 in which it is heated, as by means of steampassing through a pipe 3 disposed within the reservoir. The material maybe heated to any degree before carbonization occurs and simultaneouslywith the heating, currents of air under ressure are passed through oneor more pipes 4 and thence through nozzles 5 thereon so as to bedischarged into the mass in the reservoir in a finally divided conditionto dehydrogenate the mass. This dis-hydrogenated mass then has a solventsuch as benzin, petroleum oils, or tar oils admitted thereto, as througha pipe 6, in order to separate the insoluble portion of the material(consisting of strongly dehydrogenated substances) from the solubleportion. The material may now be decanted as through a pipe 7 whichconveys it to a still 8. A cut of! valve 9 is provided in while 'in arent ofoxidizing gaseous matter, adding-a pipe 7 and is opened to permitthe liquid to flow, therethrough, after which it is closed. The oxidizedmass of insoluble dehydrogenated hydrocarbon remaining in the still isthen heated by 'the oughly carbonized and the-carbon product sought isobtained. Asto the decanted material in the still 8, the same isdistilled while therein and the solvent separated so that the dissolvedsubstances obtained as tioned.

lrVhat Iclaim is 1. A process for the production of carbon consisting intreating hydrocarbons residue may be utilized'as hereinbefore men--while in a heated state -with-- an oxidizing current of gaseous matterto a degree short of carbonizing the hydrocarbons-subsequently treatingthe, hydrocarbons with a solvent in order to separate dehydrogenatedinsoluble substances contained in the oxidized mass, and-subsequentlycarbonizing the insoluble mass toproduce the ultimate product P L f 2. Aprocess for' the ,productionof carbon consisting in treatinghydrocarbons heated state with a divided curpipe 3 until it istliorsolvent to the oxidized material, separating the soluble substancesfrom the remainder of the oxidized materials, heating the said solubleremainder, treating said remainder with a current of oxidizing gas, andcarbonizing the dehydrogenated insoluble sub stances obtained.

3. A processfor the production of carbon consisting in treatinghydrocarbons while in a heatedstate with oxidizing gaseous matter,adding a solvent thereto, to sep arate the insoluble substances obtainedby this oxidation, separating the soluble part of the. oxidized massobtained from the insoluble substances and mixing the same with rawhydrocarbons, 'trea.ting the latter mixtnre with a current of oxidizinggaseous matter until the mixture has been transformed into a masscontaining a substan: tiab proportion of strongly dehydrogenat-edinsoluble substances, and car'bonizing the dehydrugenated insolublesubstances.

In testimony whereof I affix my signature in presenceof two witnesses.

HENRI HENNEBUTTE.

Witnesses:

CHAS. P. PnEssLY, S; MOSLEY.

